反应详情

温度

20 °C

A round-bottomed flask equipped with a magnetic stirrer was added (2S,3R)-4-benzyl-2-methyl-5-oxomorpholine-3-carboxylic acid (1 g, 4.01 mmol), EtOH (20 ml), thionyl chloride (1.155 ml, 16.05 mmol). The reaction was stirred at 20° C. for 72 hours. Concentrate in vacuo to afford a crude oil. The oil was purified by silica gel column chromatography (eluting with 20% EtOAc in Hexanes using the Moritex SI-60 size 60—half column). The resultant fractions were collected and concentrated in-vacuo to afford (2S,3R)-ethyl 4-benzyl-2-methyl-5-oxomorpholine-3-carboxylate (683 mg, 2.46 mmol, 61.4% yield) as a white solid. MS [M+H] found 278.

1. customA round-bottomed flask equipped with a magnetic stirrer
2. concentrationConcentrate in vacuo
3. customto afford a crude oil
4. customThe oil was purified by silica gel column chromatography (
5. washeluting with 20% EtOAc in Hexanes using the Moritex SI-60 size 60—half column)
6. customThe resultant fractions were collected
7. concentrationconcentrated in-vacuo